Research on the Determination of 14 Synthetic Musks in Sediment Samples by Gas Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction

TONG Ling; TIAN Qin; YANG Zhi-peng; PAN Meng

doi:10.15898/j.cnki.11-2131/td.201906240089

TONG Ling, TIAN Qin, YANG Zhi-peng, PAN Meng. Research on the Determination of 14 Synthetic Musks in Sediment Samples by Gas Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction[J]. Rock and Mineral Analysis, 2020, 39(4): 587-596. DOI: 10.15898/j.cnki.11-2131/td.201906240089

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Research on the Determination of 14 Synthetic Musks in Sediment Samples by Gas Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction

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BACKGROUNDIn recent years, the pollution of synthetic musk in the environment has increased. This kind of material has potential carcinogenic and environmental hormone effects and poses a threat to human health. Therefore, it has attracted increasing attention from scientists. The analytical technology of synthetic musk in environmental samples such as water and soil has developed rapidly. The concentration of synthetic musk in sediments has reached several thousand ng/g, but the methods for the simultaneous extraction and purification and rapid analysis of various types of synthetic musk in complex matrices of sediments are yet to be studied.OBJECTIVESTo establish a rapid method for the analysis of 14 typical synthetic musks in sediment samples by accelerated solvent extraction (ASE) combined with gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS).METHODSAccelerated solvent extraction was used for sample preparation. The ASE cell was filled up with sorbent (0.4g GCB combined with 1.0g SAX) and 5.0g sediment samples. The sample was extracted in two cycles with mixed solvents hexane-acetone (V/V, 4:1) at 80℃. After preconcentration, the extracted solution was determined by GC-MS/MS.RESULTSThe linear range of this method for fourteen target compounds ranged from 5ng/mL to 200ng/mL. The average spike-added recoveries ranged from 70.6% to 121.5%, the relative standard deviations (RSD, n=7) were 0.97%-19.5%. The recoveries of surrogates were 72.2%-116.8%. The detection limits of the method were 0.10-0.19ng/g for nitro musk, 0.09-0.14ng/g for polycyclic musk, and 0.11-1.93ng/g for macrocyclic musk.CONCLUSIONSThis method can satisfy the analysis of musk in sediments with complex matrices.

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Research on the Determination of 14 Synthetic Musks in Sediment Samples by Gas Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction

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